US7468095B2 - System for controlling flow into chromatographic column using transfer line impedance - Google Patents

System for controlling flow into chromatographic column using transfer line impedance Download PDF

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Publication number
US7468095B2
US7468095B2 US11/432,158 US43215806A US7468095B2 US 7468095 B2 US7468095 B2 US 7468095B2 US 43215806 A US43215806 A US 43215806A US 7468095 B2 US7468095 B2 US 7468095B2
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pressure
transfer line
outlet
inlet
column
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US20060260383A1 (en
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Andrew Tipler
Richard G Edwards
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PerkinElmer US LLC
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PerkinElmer LAS Inc
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Priority to US11/432,158 priority Critical patent/US7468095B2/en
Application filed by PerkinElmer LAS Inc filed Critical PerkinElmer LAS Inc
Priority to JP2008511474A priority patent/JP4768810B2/ja
Priority to EP06770425.4A priority patent/EP1880202B1/en
Priority to PCT/US2006/018890 priority patent/WO2006124877A1/en
Publication of US20060260383A1 publication Critical patent/US20060260383A1/en
Priority to US12/332,539 priority patent/US7691181B2/en
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Assigned to PERKINELMER U.S. LLC reassignment PERKINELMER U.S. LLC ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: PERKINELMER HEALTH SCIENCES INC.
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
    • G01N2030/324—Control of physical parameters of the fluid carrier of pressure or speed speed, flow rate
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/86—Signal analysis
    • G01N30/8693—Models, e.g. prediction of retention times, method development and validation

Definitions

  • the present invention relates to systems and methods for controlling the flow rate of fluid into a chromatographic column. More specifically, the invention relates to systems and methods that include controlling the flow rate of the fluid based on the impedance of a transfer line used to communicate the fluid to the column.
  • Gas chromatography is essentially a physical method of separation in which constituents of a vapor sample in a carrier gas are adsorbed or absorbed and then desorbed by a stationary phase material in a column.
  • a pulse of the sample is introduced into a steady flow of carrier gas, which carries the sample into a chromatographic column.
  • the inside of the column is lined with a liquid, and interactions between this liquid and the various components of the sample—which differ based upon differences among partition coefficients of the elements—cause the sample to be separated into the respective elements.
  • the individual components are more or less separated in time.
  • Detection of the gas provides a time-scaled pattern, typically called a chromatogram, that, by calibration or comparison with known samples, indicates the constituents, and the specific concentrations thereof, which are present in the test sample.
  • a time-scaled pattern typically called a chromatogram
  • a fluid source such as a carrier gas supply and/or a sampling device, such as a headspace sampler or thermal desorption unit, is connected to the chromatographic column via a transfer line.
  • This transfer line which may, for example, comprise a length of fused silica tubing, communicates the fluid from the source to the column for separation and detection.
  • an additional device may also be provided for performing some additional pre-concentration of analytes, such as in the system disclosed in U.S. Pat. No. 6,652,625 to Tipler, the contents of which are herein incorporated by reference in their entirety.
  • ⁇ c ⁇ 0 ⁇ ( T c T 0 ) x ( 1 ) where: ⁇ c is the viscosity at column temperature T c
  • F o ⁇ ⁇ d c 4 ⁇ ( P i 2 - P o 2 ) 256 ⁇ L c ⁇ ⁇ c ⁇ P o ( 2 )
  • F o is the flow rate at the column outlet
  • Some gas chromatographs are equipped with electronic programmable pneumatic controls. Therefore, because the relationship between viscosity and temperature is well known as described above, and because the GC oven temperature is known due to the fact that it is controlled by the same system, the chromatograph is able to readily compensate for the above-described changes in gas viscosity by increasing the column inlet pressure at a rate calculated to maintain a constant (isochoric) flow rate through the column.
  • the gas pressure is controlled on a device remote from the chromatograph, such as a sampling device.
  • a sampling device This requires that the sampling device have constant knowledge of the column temperature in order to calculate the viscosity at that temperate and make the appropriate adjustments to the applied pressure.
  • a temperature sensor may be employed to measure the temperature of the column and communicate this measurement to the sampling device, and the sampling device then adjusts the pressure at which it supplies the fluid based, in part, upon this temperature.
  • the sampling device In order to effect the above-described pressure compensatory approach, the sampling device must know the geometry and temperature of both the transfer line and the column, unless the pressure is controlled at an interface between the two. In some cases, an interface device is employed to control the flow rate of the fluid flowing into the chromatographic column.
  • an interface device is employed to control the flow rate of the fluid flowing into the chromatographic column.
  • the present teachings include systems and methods for controlling the flow rate of a fluid into a chromatographic column such that a substantially constant flow rate through the column is maintained as the column temperature changes. Further, systems and methods are provided for controlling the flow rate of a fluid into a chromatographic column that does not require knowledge of the geometry and temperature of both the transfer line and the column. Additionally, systems and methods are provided for controlling the flow rate of a fluid into a chromatographic column that does not require an additional interface device.
  • the invention comprises a method for controlling the flow into a chromatographic column, including communicating a fluid through a transfer line to a chromatographic column, determining the inlet pressure at an inlet end of the transfer line, determining the outlet pressure at an outlet end of the transfer line, and adjusting the pressure at the inlet end of the transfer line to produce a desired flow rate at the outlet end of the transfer line based on the determined inlet and outlet pressures.
  • the invention comprises a method for controlling the flow into a chromatographic column, including receiving the gas supplied by the sampling device, providing a transfer line through which the gas is communicated from the sampling device to the column and through which the gas flows from a inlet end to an outlet end, selecting a desired flow rate for the fluid flowing out of the transfer line and into the column, determining the pressure at the inlet end of the transfer line, determining the pressure at the outlet end of the transfer line, and adjusting the pressure at the inlet end of the transfer line until the determined inlet and outlet pressures produce the desired flow rate for the fluid flowing into the column.
  • the inlet pressure is adjusted by adjusting a proportional valve.
  • the inlet pressure is determined by measuring the pressure at the inlet end of the transfer line with a pressure transducer.
  • the outlet pressure is determined by measuring the pressure difference across the transfer line (e.g., between the inlet and the outlet) with a differential pressure transducer, and then calculating the outlet pressure from the measured inlet pressure and the measured pressure difference.
  • the outlet pressure is determined by measuring the pressure at the outlet end of the transfer line with a pressure transducer.
  • the invention further includes calculating an expected pressure difference across the column (e.g., between the inlet and the outlet) at the desired flow rate, measuring the actual pressure difference across the column, and comparing the expected pressure difference to the actual pressure difference.
  • the invention comprises a system for controlling the flow into a chromatographic column, including a transfer line that communicates a fluid to a chromatographic column, the transfer line having an inlet end and an outlet end, a valve that controls the pressure of the fluid at the inlet end of the transfer line, a first pressure transducer that measures the pressure at the inlet end of the transfer line, a second pressure transducer for determining the pressure at the outlet end of the transfer line, and a controller that receives signals from the first and second transducers and, in response thereto, adjusts the valve to establish a desired flow rate at the outlet end of the transfer line.
  • the invention includes a heating assembly in which the transfer line is disposed for controlling the temperature of the transfer line.
  • the sampling device is a headspace sampler, while in other embodiments, the sampling device is a thermal desorption unit.
  • FIG. 1 is schematic view of sampling system in accordance with one embodiment of the invention.
  • FIG. 2 is a schematic view of the use of pressure difference measurements to control the flow rate in a system according to FIG. 1 .
  • FIG. 3 is a schematic view of the use of outlet pressure measurements to control flow rate in a system according to FIG. 1 .
  • FIGS. 1-2 The basic components of one embodiment of a system for controlling flow rate into a chromatographic column in accordance with the invention are illustrated in FIGS. 1-2 .
  • the terms “top,” “bottom,” “above,” “below,” “over,” “under,” “above,” “beneath,” “on top,” “underneath,” “up,” “down,” “upper,” “lower,” “front,” “rear,” “back,” “forward” and “backward” refer to the objects referenced when in the orientation illustrated in the drawings, which orientation is not necessary for achieving the objects of the invention.
  • the system 10 includes a source of fluid, such as sampling device 20 , which, in the particular embodiment described below, is a thermal desorption unit, but, in other embodiments, may include other sampling devices, such as a headspace sampler.
  • the system 10 further includes a gas chromatograph 22 , which includes a chromatographic column 24 connected to a detector 26 .
  • the thermal desorption unit 20 is in fluid communication with the chromatograph 22 via a transfer line 28 , through which a sample mixture is communicated from the unit 20 to the column 22 (indicated by arrows A).
  • the transfer line 28 comprises a length of tubing having two ends, where one of such ends is referred to herein as a transfer line outlet that is in fluid communication with the column 24 at a point that is referred to herein as the column inlet. Similarly, the other end of the transfer line 28 can be referred to as the transfer line inlet.
  • the transfer line 28 can be made from an inert material, such as, for example, deactivated fused silica or silica-coated stainless steel tubing, although such examples are provided for illustration and not limitation. In some embodiments, the transfer line 28 is between about one and two meters long and has an internal diameter of less than 0.5 mm. Such tubing can be made with a reasonable tolerance, and thus, the internal geometry of the transfer line 28 is predictable.
  • the flow rate through the transfer line 28 is often the same as the flow rate through the column 24 . In the case of capillary columns, this will sometimes mean a flow rate of less than 1 mL/min.
  • the pressure at which the fluid must be applied in order to achieve a desired flow rate at the transfer line outlet can be determined by using the Hagen-Poiseuille equation (Equation 2) for the transfer line (as opposed to the column), which can be simplified to:
  • the transfer line 28 is surrounded by a concentric heating assembly 30 , which prevents possible condensation of the sample material flowing through it.
  • the heating assembly 30 can extend along the entire length of the transfer line 28 .
  • the heating assembly 30 may comprise an inner, slightly rigid, stainless steel tube, approximately an eighth of an inch in diameter, through which the transfer line 28 is threaded, and a resistive heating coil wound around this tube. Insulators may then be provided around this coil, such as, for example, a fiber glass webbing, which may, in turn, be surrounded by an insulative foam. The temperature of the heater is normally controlled, and thus, the transfer line 28 can be maintained at a constant temperature.
  • the aforementioned pressure difference can be assessed as illustrated in FIG. 2 .
  • a fluid source such as the carrier gas supply 38 illustrated in FIG. 2 , supplies fluid through a proportional valve 40 .
  • a first pressure transducer 42 measures the pressure at the transfer line inlet 52 , and communicates this pressure P i to a controller 50 .
  • a second absolute transducer 46 can be employed to measure the outlet pressure P o instead of using the differential pressure transducer described above.
  • the differential transducer 44 configuration shown in FIG. 2 due to the relative magnitudes of large pressures and small pressure differences, it can be useful to employ the differential transducer 44 configuration shown in FIG. 2 .
  • the controller 50 uses the measured values of P i and P o to adjust the proportional valve 40 until the measured/calculated inlet and outlet pressures, when considered with respect to Equation 3, produce the desired flow rate F o for the transfer line outlet (column inlet). If the temperature changes, so will the viscosity and the flow rate, and therefore, the illustrated systems and methods allow for adjustments to be made to the applied pressure to compensate for such changes.
  • the inlet pressure P i is adjusted directly by the proportional valve 40 , while the pressure difference ⁇ P, while measurable, is not directly controlled.
  • the main electronic/firmware control loop i.e., inner loop
  • the outlet pressure or the difference in pressure, from which the output pressure is calculated
  • the proportional valve 40 will be adjusted until the combination of P i and ⁇ P produces the correct flow rate F o according to Equation 3.
  • Equation 3 The efficacy of the calculations resulting from the use of Equation 3 will depend on how accurately the geometry and temperature of the transfer line is defined. In practice, the internal diameter and exact temperature of the transfer line can be difficult to measure, and thus, in some cases, a system calibration may be performed. Accordingly, Equation 3 can be modified to:
  • the values for F o will be for the volumetric flow rate at the temperature and pressure at the outlet of the transfer line. Because this will normally be at an elevated temperature and possibly at a pressure different from ambient, the values for F o must be corrected to the flow rate measurements expected by the user, as it is typical practice to express (and apply) the flow rate corrected to Standard Ambient Temperature and Pressure (SATP), as shown below:
  • SATP Standard Ambient Temperature and Pressure
  • F a F o ⁇ P o P a ⁇ T o T a ( 6 ) where: F a is the flow rate corrected to SATP
  • the above-described system permits an operator to control flow rate into a column without knowledge of the temperature or geometry of the column itself, in the event that these column parameters are known, the above described system can be further utilized to test for possible leaks and/or blockages.
  • the pressure difference across the column 24 can be predicted for a given flow rate. This predicted pressure difference can be compared to an actual pressure difference across the column 24 as the flow rate is being controlled as described above. If more than an insignificant difference is detected between the predicted and actual pressure differences, this would indicate the possible presence of a leak at the connection between the transfer line 28 and column 24 or a blockage in the transfer line or column.

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US11/432,158 US7468095B2 (en) 2005-05-12 2006-05-11 System for controlling flow into chromatographic column using transfer line impedance
JP2008511474A JP4768810B2 (ja) 2005-05-12 2006-05-12 トランスファー・ライン・インピーダンスを使用してクロマトグラフィーコラム内への流れを制御するためのシステム
EP06770425.4A EP1880202B1 (en) 2005-05-12 2006-05-12 Method for controlling flow into chromatographic column using transfer line impedance
PCT/US2006/018890 WO2006124877A1 (en) 2005-05-12 2006-05-12 System for controlling flow into chromatographic column using transfer line impedance
US12/332,539 US7691181B2 (en) 2005-05-12 2008-12-11 System for controlling flow into chromatographic column using transfer line impedance

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US8562837B2 (en) 2010-09-22 2013-10-22 Perkinelmer Health Sciences, Inc. Backflush methods and devices for chromatography
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JP4768810B2 (ja) 2011-09-07
JP2008541097A (ja) 2008-11-20
WO2006124877A1 (en) 2006-11-23
US20090084261A1 (en) 2009-04-02
US7691181B2 (en) 2010-04-06
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WO2006124877B1 (en) 2007-04-05

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